CN110382730A - The manufacturing method and sprayed manufacturing method of sprayed, spraying plating powder, spraying plating powder - Google Patents
The manufacturing method and sprayed manufacturing method of sprayed, spraying plating powder, spraying plating powder Download PDFInfo
- Publication number
- CN110382730A CN110382730A CN201880014710.6A CN201880014710A CN110382730A CN 110382730 A CN110382730 A CN 110382730A CN 201880014710 A CN201880014710 A CN 201880014710A CN 110382730 A CN110382730 A CN 110382730A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- earth element
- spraying plating
- powder
- fluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims description 191
- 238000007747 plating Methods 0.000 title claims description 159
- 238000005507 spraying Methods 0.000 title claims description 155
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 136
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 74
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 claims abstract description 40
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 21
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 20
- 239000011733 molybdenum Substances 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 54
- 239000007789 gas Substances 0.000 claims description 50
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 47
- 239000001301 oxygen Substances 0.000 claims description 47
- 229910052760 oxygen Inorganic materials 0.000 claims description 47
- 229910052751 metal Inorganic materials 0.000 claims description 45
- 239000002184 metal Substances 0.000 claims description 45
- 229910052782 aluminium Inorganic materials 0.000 claims description 43
- 229910052726 zirconium Inorganic materials 0.000 claims description 43
- 229910052738 indium Inorganic materials 0.000 claims description 42
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 39
- 239000002131 composite material Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 27
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 24
- 229910052727 yttrium Inorganic materials 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 3
- -1 rare earth fluoride Chemical class 0.000 abstract description 20
- 238000004140 cleaning Methods 0.000 abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 34
- 229910052786 argon Inorganic materials 0.000 description 17
- 229940105963 yttrium fluoride Drugs 0.000 description 16
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 description 16
- 229910000838 Al alloy Inorganic materials 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 14
- 239000001257 hydrogen Substances 0.000 description 14
- 229910052739 hydrogen Inorganic materials 0.000 description 14
- 238000007750 plasma spraying Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000007921 spray Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002845 discoloration Methods 0.000 description 6
- 238000005453 pelletization Methods 0.000 description 6
- 238000001020 plasma etching Methods 0.000 description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000003682 fluorination reaction Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 229930006000 Sucrose Natural products 0.000 description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 3
- 229920005822 acrylic binder Polymers 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UOBPHQJGWSVXFS-UHFFFAOYSA-N [O].[F] Chemical compound [O].[F] UOBPHQJGWSVXFS-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- TYIZUJNEZNBXRS-UHFFFAOYSA-K trifluorogadolinium Chemical compound F[Gd](F)F TYIZUJNEZNBXRS-UHFFFAOYSA-K 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910015221 MoCl5 Inorganic materials 0.000 description 1
- VSOYJNRFGMJBAV-UHFFFAOYSA-N N.[Mo+4] Chemical compound N.[Mo+4] VSOYJNRFGMJBAV-UHFFFAOYSA-N 0.000 description 1
- ZWNZGTHTOBNSDL-UHFFFAOYSA-N N.[Ti+4] Chemical compound N.[Ti+4] ZWNZGTHTOBNSDL-UHFFFAOYSA-N 0.000 description 1
- 241000227425 Pieris rapae crucivora Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010062 TiCl3 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/259—Oxyhalides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/5156—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on rare earth compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32458—Vessel
- H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Abstract
It provides sprayed, is sprayed, the titanium or molybdenum of carbon or 1~1000ppm containing 0.01~2 mass % comprising rare earth fluoride and/or rare earth oxygen fluoride, and in the case where being free of oxygen fluoride, use L*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+5.0, b*Grey or even black for -4.0~+8.0 use L comprising oxygen fluoride*a*b*Chrominance representation is in L*It is 25 or more and less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even black.If the envelope is formed in anti-plasma member, the color of part it is with low uncertainty, also need not partly implement the cleaning for being difficult to carry out again when taking out cleaning, become the component that can realize the long-life of script really.
Description
Technical field
The present invention relates to the oxygen fluorine of the fluoride comprising the fluoride of rare earth element or the rare earth element and rare earth element
The sprayed manufacturing method for obtaining the sprayed spraying plating powder, the spraying plating powder of compound and this is sprayed
Manufacturing method.
Background technique
In recent years, since rare earth fluoride is more stable at high temperature, in order to by being used in anti-plasma member
The long lifetime for realizing embryonic particle reduction, component using rare earth fluoride on the way, has carried out foring rare earth fluoride
The exploitation of sprayed component.The plasma-etching apparatus component of halogen gas is for example, used.
But it is white usually as the yttrium fluoride of the representative of rare earth fluoride, therefore for having used halogen gas
For plasma-etching apparatus component, the residue attachment of resist decomposition product after use, generating discoloration is dark brown part.
In addition, due to the influence of plasma etching, there is a phenomenon where partly from white discoloration be black (Hall caused by color center
Defect etc.), thus emphasis clean the part, as a result there are the following problems: there is plasma-resistance originally and can be long-lived
Lifeization but makes service life reduction by cleaning.It should be noted that as existing technical literature, can enumerate following patent documents 1~
6。
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2004-100039 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2012-238894 bulletin
Patent document 3: No. 3894313 bulletins of Japanese Patent No.
Patent document 4: Japanese Unexamined Patent Publication 2014-010638 bulletin
Patent document 5: No. 5396672 bulletins of Japanese Patent No.
Patent document 6: Japanese Unexamined Patent Publication 2016-079258 bulletin
Summary of the invention
Subject to be solved by the invention
The present invention is completed in view of above-mentioned actual conditions, and it is an object of the present invention to provide waiting the face of parts after the use of spraying plating component
Color it is consistent it is sprayed, for obtaining the sprayed spraying plating powder and the spraying plating powder, the sprayed system
Make method.
Means for solving the problems
The present inventor has made intensive studies to achieve the goals above, as a result completes the present invention.That is, above-mentioned asks
Topic is that rare earth fluoride, the rare earth fluoride comprising oxygen fluoride are substantially white, from this point, in order to which these are dilute
Native fluoride is colored as grey or black, considers addition other elements.But, for anti-plasma member, due to master
It to be used in semiconductor fabrication process, it is therefore desirable to consider this antipollution point, its additive amount also to be inhibited to have become necessary,
Therefore it is required that formed using a small amount of addition element in regulation coloration white or grey so that black rare earth fluoride,
Rare earth fluoride comprising oxygen fluoride it is sprayed.Therefore, in view of the requirement, continue to study, as a result know and especially contain
When having carbon or titanium or molybdenum, especially in the case of carbon containing 0.01~2 mass %, in the case where titanium, molybdenum containing 1~
1000ppm is effectively, further to L*a*b*Chrominance representation has carried out various researchs, as a result knows: by using with L*a*b**
Chrominance representation is in L*It is 25 or more and less than 91, sometimes 25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 white or
The spraying plating powder of the rare earth fluoride or the rare earth fluoride comprising oxygen fluoride of person's grey or even black, to can be achieved
The white or grey of the purpose of the present invention or even black it is sprayed, complete the present invention.
Therefore, as first invention, following sprayed, spraying plating powder and the spraying plating powder manufacturing methods are provided.
[1] sprayed, which is characterized in that being includes following (1) and/or (2) or following (1) and/or (2) and choosing
From the sprayed of the one kind or two or more mixture in following (3)~(5),
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
Carbon containing 0.004~2 mass % or titanium or molybdenum containing 1~1000ppm, and
In the case where being free of the oxygen fluoride of above-mentioned (2), L is used*a*b*Chrominance representation is in L*For 25~64, a*It is -3.0
~+5.0, b*Grey or even black for -6.0~+8.0,
Comprising the oxygen fluoride of above-mentioned (2), L is used*a*b*Chrominance representation is in L*For 25 or more and less than 91,
a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even black.
[2] [1] it is sprayed, wherein rare earth element is selected from one or more of Y, Gd, Yb, La.
[3] [1] or [2] it is sprayed, wherein oxygen content is 0.01~13.5 mass %.
[4] any one of [1]~[3] is sprayed, wherein carbon content is 0.004~0.15 mass %.
[5] spraying plating powder, which is characterized in that being includes following (1) and/or (2) or following (1) and/or (2) and choosing
From the spraying plating powder of the one kind or two or more mixture in following (3)~(6),
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
Carbon containing 0.004~2 mass % or titanium or molybdenum containing 1~1000ppm, and use L*a*b*Chrominance representation,
In L*It is 25 or more and less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even black.
[6] the spraying plating powder of [5], wherein rare earth element is selected from one or more of Y, Gd, Yb, La.
[7] the spraying plating powder of [5] or [6], wherein oxygen content is 0.01~13.5 mass %.
[8] the spraying plating powder of any one of [5]~[7], be the spraying plating powder through being burnt into, carbon content be 0.004~
0.15 mass %.
[9] the spraying plating powder of any one of [5]~[7], for the spraying plating powder not being burnt into, carbon content is 0.004~1.5
Quality %.
[10] manufacturing method of spraying plating powder is the method for manufacturing the spraying plating powder of any one of [5]~[8], feature
It is, will will include following (1) and/or (2) or following (1) and/or (2) and a kind or 2 kinds in following (3)~(6)
The white powder of above mixture and the carbon used in such a way that the concentration of carbon of spraying plating powder becomes 0.004~2 mass %
The slurry in source is dry, roasting, is burnt into, and obtains using L*a*b*Chrominance representation is in L*It is 25 or more and less than 91, a*For -3.0~+5.0,
b*For -6.0~+8.0 white or grey or even the spraying plating powder of black.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
[11] manufacturing method of the spraying plating powder of [10], wherein after being roasted at 500~800 DEG C in nitrogen,
The powder being fired is burnt at 800~1000 DEG C in vacuum or non-active gas atmosphere.
[12] manufacturing method of the spraying plating powder of [10] or [11], wherein including above-mentioned (1) and/or (2) or above-mentioned
(1) and/or the oxygen content of the white powder of (2) and the one kind or two or more mixture in above-mentioned (3)~(6) is
0.01~13.5 mass %.
[13] manufacturing method of any one of [10]~[12], wherein with the concentration of carbon of spraying plating powder become 0.004~
The mode of 0.15 mass % uses carbon source.
[14] manufacturing method of spraying plating powder is the method for manufacturing the spraying plating powder of any one of [5]~[8], feature
It is, will will include following (1) and/or (2) or following (1) and/or (2) and a kind or 2 kinds in following (3)~(6)
The white powder of above mixture, polyvinyl alcohol, the side with the concentration of the titanium of spraying plating powder or molybdenum as 1~1000ppm
The slurry granulating and drying of the water soluble salt of titanium or molybdenum that formula uses, firing, obtain using L*a*b*Chrominance representation is in L*For 25 or more and
Less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even the spraying plating powder of black.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
[15] manufacturing method of the spraying plating powder of [14], wherein 800~1000 in vacuum or non-active gas atmosphere
The powder through granulating and drying is burnt at DEG C.
[16] manufacturing method of the spraying plating powder of [14] or [15], wherein including above-mentioned (1) and/or (2) or above-mentioned
(1) and/or the white powder including mixture of (2) and the one kind or two or more mixture in above-mentioned (3)~(6)
Oxygen content be 0.01~13.5 mass %.
In addition, the research of the present inventor's further progress, as a result, it has been found that: even if carbon-free in envelope, titanium or molybdenum, can also adopt
Make envelope surface due to color center and grey or even blackened with plasma light and reaction gas, by using plasma in advance
Body exposure treatment makes envelope surface grey or even blackened, thus in the sputtered films of bismuth for the component that plasma-etching apparatus is made
In the case where will not generate because of caused by use discoloration, it can be achieved that aforementioned present invention purpose.
Therefore, as the second invention, the following sprayed and sprayed manufacturing method is provided.
[17] sprayed, which is characterized in that being includes following (1) and/or (2) or following (1) and/or (2) and choosing
From the sprayed of the one kind or two or more mixture in following (3)~(5), have on surface and use L*a*b*Chrominance representation is in
L*For 25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 grey or even the grey of black or even black layer.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
[18] [17] it is sprayed, wherein grey or even the depth of black layer are within 2 μm away from envelope surface.
[19] [17] or [18] it is sprayed, wherein oxygen content is 0.01~13.5 mass %.
[20] sprayed manufacturing method is the sprayed manufacturing method of any one of [17]~[19], special
Sign is, will include following (1) and/or (2) or following (1) and/or (2) and a kind or 2 in following (3)~(6)
Kind or more mixture white powder to substrate surface spraying plating, obtain using L*a*b*Chrominance representation is in L*For 81 or more, a*For-
3.0~+3.0, b*For -3.0~+3.0 white it is sprayed, to the sprayed implementation plasma exposure processing,
The sprayed surface, which is formed, uses L*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+5.0, b*It is -6.0~+8.0
The grey or even black layer of grey or even black.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
[21] the sprayed manufacturing method of [20], wherein make grey or even the depth of black layer away from envelope surface
2 μm within.
[22] manufacturing method of the spraying plating powder of [20] or [21], wherein including above-mentioned (1) and/or (2) or above-mentioned
(1) and/or the oxygen content of the white powder of (2) and the one kind or two or more mixture in above-mentioned (3)~(6) is
0.01~13.5 mass %.
The effect of invention
According to the present invention, due to can by the white of regulation coloration or grey or even black comprising rare earth fluoride or
The sprayed of the rare earth fluoride of oxygen fluoride is formed a film by atmosphere plasma spraying plating, therefore cost effective is possibly realized.
In addition, being in the white of regulation coloration or the sprayed structure with rare earth fluoride spraying plating of grey or even black that will have this
In the case that part is used as the anti-plasma member in halogen gas, the color of part it is with low uncertainty, take out cleaning when
Without the cleaning for partly implementing to be difficult to carry out, become the component that can certainly realize the long-life of script.
Detailed description of the invention
Fig. 1 is the explanatory diagram for illustrating the measuring method of thickness of sprayed black layer.
Fig. 2 is the coordinate diagram for indicating the relationship of the sprayed carbon content and hardness in experimental example.
Specific embodiment
The present invention is described in more detail below.
In above-mentioned first invention, it is of the invention it is sprayed be include following (1) and/or (2) or following (1) and/
Or (2) and the one kind or two or more mixture in following (3)~(5) is sprayed.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
In addition, it includes following (1) and/or (2) or following (1) and/or (2) and be selected from that spraying plating of the invention is with powder
The spraying plating powder of one kind or two or more mixture in following (3)~(6).
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
In this case, as above-mentioned rare earth element, as described above, can be from the rare earth element of the 3A race comprising yttrium (Y)
It is middle to use a kind or more, in particular it is preferred to for the one kind or two or more heavy rare earth element in Y, Gd, Yb and La.Wherein,
The oxygen fluoride of rare earth element as above-mentioned (2) is able to use the oxygen fluoride of various crystalline textures, such as the oxygen fluorine in Y
In the case where compound, it is able to use Y5O4F7、Y6O5F8, the various crystalline textures such as YOF oxygen fluoride.
The average grain diameter of the particle of spraying plating powder in the present invention is preferably 1~100 μm, if average grain diameter less than 1 μm,
It is possible that evaporating, dispersing in plasma flame in spraying plating etc., loss is correspondingly generated.On the other hand, if average grain diameter
More than 100 μm, it is possible to not melted fully in plasma flame in spraying plating etc. and melt incomplete, become and do not melt
Powder, it is possible to incur the reduction of dhering strength.It should be noted that above-mentioned average grain diameter is the granularity point using laser diffractometry measurement
The value of the D50 of cloth.
Sprayed and spraying plating of the invention is containing to usually white rare earth fluoride powder (such as L with powder*: 91
Above, a*: -3.0~+3.0, b*: -3.0~+3.0 fluorination yttrium powder etc.), rare earth fluoride powder comprising oxygen fluoride assign ash
The material of color or even black and prepare so that become L*It is 25 or more and less than 91, a*For -3.0~+5.0, b*It is -6.0~+8.0
L*a*b*Chrominance representation.But, about above-mentioned L*Value, in the envelope of the oxygen fluoride for the rare earth element without above-mentioned (2)
In the case where, it is set as L*: 25~64.As above-mentioned imparting grey or even the material of black, such as using carbon, titanium, molybdenum, especially
In the case of carbon, preferably make in envelope or powder containing it so that becoming 0.004~2 mass %, particularly 0.05~1.8 matter
% is measured, in addition, preferably comprising it so that becoming 1~1000ppm, particularly 1~800ppm in the case where titanium, molybdenum.In addition,
In the present invention, to sprayed and spraying plating powder oxygen content, there is no particular restriction, preferably 0.01~13.5 mass %, more
Preferably 0.05~8 mass %.
Here, the understanding of people according to the present invention, above-mentioned carbon content influences the hardness of envelope sometimes, if carbon content increases,
Sometimes the hardness of envelope reduces.Therefore, need height by film hardness in the case where, preferably make carbon content become 0.15 mass % with
Under, especially 0.1 mass % or less.Further more, the lower limit value of carbon content is as described above, be 0.004 mass %, preferably 0.01 matter
Measure %, more preferably 0.02 mass %.Quilt thus, it is possible to the hardness for obtaining that there is 300HV or more, particularly 400HV or more
Film.When obtaining the envelope of such high rigidity, in the case where the spraying plating powder through being burnt into, carbon content can be made to become 0.004
~0.15 mass %, in the case where the spraying plating powder not being burnt into, can make carbon content become 0.004~1.5 mass %, pass through by
Such spraying plating powder spraying plating, so as to obtain 0.15 mass % of the carbon content spraying plating below with above-mentioned good hardness
Envelope.
As the means for containing above-mentioned carbon, there is no particular restriction, such as following method can be used: use is comprising by above-mentioned
(1) and/or (2) or above-mentioned (1) and/or (2) are constituted with the one kind or two or more mixture in above-mentioned (3)~(6)
The solution of white powder and carbon source prepare slurry, mixing 5~dry after sixty minutes is granulated, firing.In this case, make
For carbon source, carbon, aliphatic hydrocarbon, aromatic hydrocarbon etc. can be used, it can be made to dissolve and mix in water, organic solvent as needed
It closes, such as is able to use that (such as acrylic binder, carboxymethyl are fine by the diluted product of phenol alcohol, water soluble organic substance
Tie up element (CMC), polyvinyl alcohol (PVA), sucrose), become carbon source as long as being burnt into, it's not limited to that.For carbon addition,
Directly mixing, dipping, coating, injection etc. can be used.After carbon source is mixed with above-mentioned powder, is dry, preferably 500 in nitrogen
It is burnt at~1000 DEG C.After firing, by being sieved, thus obtain presenting above-mentioned regulation coloration white or grey or even
The spraying plating powder of black.In addition, can also make to mix without firing after mixing with above-mentioned powder by above-mentioned carbon source, dry, be granulated
Xeraphium is directly as spraying plating powder.In turn, the spraying plating for using partial size tiny as SPS (suspension plasma spray coating) slurry is used
In the case where powder (1~10 μm), dry, granulation is not needed.
When obtaining spraying plating powder in this way, in this invention it is important that control becomes the phenol of carbon source, acrylic acid series bonding
The addition concentration of agent, CMC, PVA, sucrose etc. is so that the concentration of carbon in spraying plating powder becomes 0.004~2 mass %.If carbon contains
Amount cannot get the coloring film of target less than 0.004 mass %, in high temperature firing, powder weakened when spraying plating, sometimes in powder
It is generated in performance uneven.On the other hand, if carbon content is more than 2 mass %, the excessive concentration of carbon and become surplus materials, lead more
Pollution, sprayed hardness is caused to reduce.Further more, there is such as 300HV or more, particularly 400HV in order to be made as described above
The envelope of above high rigidity, in the case where the spraying plating powder through being burnt into, preferably the addition concentration of control carbon source is so that spraying plating is used
The carbon content of powder becomes 0.004~0.15 mass %, particularly 0.01~0.1 mass %, in the feelings for the spraying plating powder not being burnt into
Under condition, preferably the addition concentration of control carbon source is so that carbon content becomes 0.004~1.5 mass %.
In addition, there is no particular restriction as the means containing titanium, molybdenum, such as following method can be illustrated: will be by above-mentioned
(1) and/or (2) or above-mentioned (1) and/or (2) are constituted with the one kind or two or more mixture in above-mentioned (3)~(6)
White powder, polyvinyl alcohol (PVA), water, titanium or the water-soluble salt such as titanium chloride, titanium ammonium, molybdenum chloride, molybdenum ammonium of molybdenum etc.
Mixing, is made slurry, using spray dryer granulating and drying.In turn, by by the powder in vacuum or non-active gas atmosphere
It is burnt at 800 DEG C or more and 1000 DEG C or less, so as to obtain the spraying plating powder of grey or even black.At this point, titanium or molybdenum
Content is set as 1~1000ppm.If the content of titanium or molybdenum cannot get the coloring film of target less than 1ppm, in addition, if it exceeds
1000ppm, especially used in the semiconductor manufacturing apparatus the reason of being likely to become pollution.
It is of the invention sprayed to send out above-mentioned for example, by substrates such as components in plasma-etching apparatus
Bright spraying plating powder spraying plating is to form a film to be formed.Here, be not particularly limited as substrate, be able to use with Al, Fe, Si,
Cr, Zn, Zr or Ni as principal component metal, alloy, ceramics metal nitride, metal carbides, metal oxide (such as
Aluminium oxide, aluminium nitride, silicon nitride, silicon carbide etc.) }, glass (quartz glass etc.) etc..
Sprayed thickness of the invention can wait depending on the application suitably to be set, and there is no particular restriction, in order to assign
Corrosion resistance and in the case where the corrosion resistance component of plasma-etching apparatus etc. forms a film as anti-corrosion envelope, preferably 50~
500 μm, more preferably 150~300 μm.If the thickness of envelope is less than 50 μm, it is possible to since the corrosion of very little just needs more
It changes.On the other hand, blocked up, it is possible to become easy peeling-off if the thickness of envelope is more than 500 μm.
It is of the invention it is sprayed can by above-mentioned substrate surface by the spraying plating of aforementioned present invention with powder using etc. from
The suitable spraying plating mode such as daughter spraying plating, reduced pressure plasma spraying plating, SPS spraying plating carries out spraying plating and is formed.In this case, make
It for plasma gas, is not particularly limited, is able to use nitrogen/hydrogen, argon/hydrogen, argon/helium, argon/nitrogen, argon/hydrogen/nitrogen etc..It should say
It is bright, spraying plating condition etc. is not particularly limited, can according to the specific material of substrate, rare earth fluoride spraying plating powder etc.,
To the purposes etc. of spraying plating component suitably set.
Obtain in this way of the invention sprayed as described above, the rare earth element without above-mentioned (2) oxygen fluoride
In the case where, use L*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 grey or even black
Color.In addition, using L in the case where the oxygen fluoride of the rare earth element comprising above-mentioned (2)*a*b*Chrominance representation is in L*It is 25 or more
And less than 91, preferably 25~85, more preferable 25~80, a*For -3.0~+5.0, b*It is for -6.0~+8.0 white or grey
To black.It is formed in L in this way*a*b*The white or grey of clear stipulaties or even black is sprayed in chrominance representation,
To need not also implement the cleaning for being difficult to carry out of the part when taking-up of treated object is cleaned again, becomes and can be realized script
The component of long-life.It should be noted that in the present invention, L*a*b*Coloration is able to use such as Minolta colour difference meter (CHOROMA
METER) CR-200, according to JIS Z 8729 measure.
It is of the invention it is sprayed in, will only the fluoride of the rare earth element comprising above-mentioned (1) spraying plating powder for example
YF3In the case where spraying plating powder spraying plating, YF has been obtained3The grey of individual crystalline texture or even black it is sprayed.Another party
Face, by be mixed in the fluoride of the rare earth element of above-mentioned (1) oxygen fluoride of the rare earth element of above-mentioned (2), (3) it is dilute
Spraying plating powder made of the oxide of earth elements, such as in YF3It is middle by Y oxygen fluoride (Y5O4F7、Y6O5F8), Y oxide (Y2O3)
In the case that the spraying plating mixed is with powder spraying plating, YF is obtained3+Y5O4F7、YF3+Y6O5F8Deng in YF3It in addition also include the Y of multiphase
The white or grey of the regulation coloration of oxygen fluoride crystalline phase or even black it is sprayed.In turn, will be in above-mentioned (1)
Spraying plating powder made of the metal oxide of above-mentioned (6) is mixed in the fluoride of rare earth element, such as in YF3In be mixed with Al
In the case where being spraying plating powder spraying plating made of oxide, YOF+Y is obtained3Al5O12+Y7O6F9、YF3+Y5O4F7+Y3Al5O12、
Y6O5F8+Y3Al5O12Deng the sprayed of the multiphase comprising fluoride, oxygen fluoride and YAG.For such sprayed
Crystalline texture can be measured using X-ray diffraction method.
In addition, for sprayed and spraying plating powder oxygen content, the oxygen content member of the rare earth as contained in raw material powder
Oxide, oxygen fluoride (such as the Y of element2O3、Y5O4F7) etc. oxygen amount determine.In the case that oxygen amount in sprayed is few,
With YF3+Y5O4F7Crystalline texture is changed into YF if oxygen amount increases3+ YOF crystalline texture.If oxygen amount further increases, have
When in YF3Y is observed other than+YOF2O3Crystalline texture.These can be confirmed using XRD diagram.In the present invention, as described above, spray
The oxygen content for plating envelope and spraying plating powder is preferably 0.01~13.5 mass %, more preferably 0.05~8 mass %, and then in oxygen
In the case that content is 6 mass % or less, particularly 2~4 mass %, it is capable of providing and 300HV or more, resistance to etc. is up to by film hardness
The presentation L that gas ions are had excellent performance*It is 25 or more and less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or
Grey or even black it is sprayed.
Wherein, the oxygen fluoride of the rare earth element of above-mentioned (2) is free of in sprayed and spraying plating powder of the invention
In the case of, as described above, L*The upper limit be set as 64.In this way by L*Value be set to it is lower, so as to further realize cleaning
The long lifetime of generation.Further more, for comprising above-mentioned (2), the oxygen fluoride of the rare earth element of (3), oxide spraying plating powder
With sprayed color, color-values L is controlled since carbon content can be used*As long as therefore L*Less than white value 91, so that it may
Arbitrarily control.It is capable of providing the white or grey or even black spraying plating powder, spraying plating quilt of regulation coloration of the invention in this way
Film.
Next, first will include following (1) and/or (2) or following (1) and/or (2) and choosing in the second invention
From the white powder of the one kind or two or more mixture in following (3)~(6) to substrate spraying plating, L is used in formation*a*b*Coloration
It indicates to be in L*For 91 or more, a*For -3.0~+3.0, b*For -3.0~+3.0 white it is sprayed.
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
Next, being formed on the sprayed surface to the sprayed implementation plasma exposure processing and using L*a*b*Color
Degree indicates to be in L*For 25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 grey or even the grey of black or even black
Layer.In this case, to the depth (thickness) away from envelope surface of above-mentioned grey or even black layer, there is no particular restriction, preferably
Within 2 μm, particularly preferably 1 μm or so.
Thus it obtains sprayed, which is characterized in that being includes following (1) and/or (2) or following (1) and/or (2)
It is sprayed with the one kind or two or more mixture in following (3)~(5),
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of above-mentioned rare earth element
(3) oxide of above-mentioned rare earth element
(4) composite oxides of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of above-mentioned rare earth element and the one kind or two or more metal in Al, Si, Zr, In exists
Surface, which has, uses L*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 grey or even black
The grey or even black layer of color.
As the processing of above-mentioned plasma exposure, as long as envelope surface grey is by using plasma light and reaction gas
Above-mentioned coloration is turned to black, can suitably set frequency, output power, the type of reaction gas, flow, gas of plasma
Body pressure etc. is so that obtain above-mentioned coloration.Other business is identical as above-mentioned first invention.It should be noted that for the above-mentioned of spraying plating
With powder, there is no particular restriction for spraying plating, and for the reason identical as above-mentioned first invention, preferably oxygen content is 0.01~13.5 matter
Measure %, more preferably 0.05~8 mass %.
Embodiment
Embodiment described below and comparative example, specifically describe the present invention, but the present invention is not by following embodiments
Limitation.It should be noted that % indicates quality % in example below.
[embodiment 1]
Addition is diluted to 3% benzene with ethyl alcohol in fluorination ytterbium (40 μm of average grain diameter) powder 1kg that oxygen concentration is 3.4%
It 1 liter of phenol solution, mixes 5 minutes, after dry, is roasted 2 hours with 800 DEG C of nitrogen streams.In turn, by the pelletizing decompression (1 ×
10-2Torr or less) under with 1000 DEG C be burnt into 2 hours, spraying plating powder is made.The spraying plating is L with powder*a*b*L in chrominance representation*:
42.3、a*: -0.30, b*: -0.65 black, the concentration of carbon in powder are 1.3%.In addition, oxygen concentration is 2.9%.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 45.2, a*: -0.53, b*: -0.62,
Concentration of carbon is 1.1%.In addition, oxygen concentration is 3.6%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[comparative example 1]
Using fluorination ytterbium (40 μm of average grain diameter) powder, it is attached to film by plasma spraying using argon gas, hydrogen
Aluminium alloy element is with the envelope as about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 91.46,
a*: -0.47, b*: 0.75, concentration of carbon 0.003%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test similarly to Example 1.Taking-up it is sprayed in see
Having arrived partly discoloration is dark brown and black part.
[embodiment 2]
By oxygen concentration be 0.2% yttrium fluoride (40 μm of average grain diameter) powder infusion in 30% aqueous solution of sucrose, stirring
After ten minutes, it filters, is dry.The yttrium fluoride powder is burnt into 2 hours with 800 DEG C of nitrogen streams, with the sieve of #100, is obtained
Spraying plating powder.The spraying plating is L with powder*a*b*L in chrominance representation*: 72.23, a*: -0.02, b*: 3.12 grey, in powder
Concentration of carbon is 0.235%.In addition, oxygen concentration is 0.75%.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 76.18, a*: 0.04, b*: 3.77,
Concentration of carbon is 0.015%.In addition, oxygen concentration is 1.1%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[embodiment 3]
In white yttrium oxide (1.1 μm of average grain diameter) powder 150g and yttrium fluoride (3 μm of average grain diameter) powder 850g
Middle 4 liters of 2% aqueous solution of addition acrylic binder simultaneously mixes, and prepares slurry, after being granulated with spray dryer, being dry,
With the sieve of #100, yttrium fluoride (36 μm of average grain diameter) powder is made, has obtained spraying plating powder.The spraying plating is L with powder*a*
b*L in chrominance representation*: 88.46, a*: 3.63, b*: -2.85 grey, the concentration of carbon in powder is 1.46%, and oxygen concentration is
3.37%.In addition, having carried out the X-ray diffraction of powder, result viewing to YF3And Y2O3Peak.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 43.18, a*: 0.87, b*: 3.78,
Concentration of carbon is 0.068 mass %, oxygen concentration 3.73%.In addition, having carried out the X-ray diffraction of envelope, result viewing to Y6O5F8
With Y5O4F7、Y2O3Peak.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[comparative example 2]
Using yttrium oxide (40 μm of average grain diameter) powder, it is attached to film by plasma spraying using argon gas, hydrogen
Aluminium alloy element is with the envelope as about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 92.75,
a*: -0.23, b*: 0.73, concentration of carbon 0.002%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr, the plasma exposure that has been performed in the same manner as in Example 2 test.Taking-up it is sprayed in see
Having arrived partly discoloration is dark brown and black part.
[embodiment 4]
In white yttrium oxide (0.2 μm of average grain diameter) powder 100g and yttrium fluoride (3 μm of average grain diameter) powder 900g
4 liters of 1% aqueous solution of middle addition carboxymethyl cellulose (CMC) binder simultaneously mixes, and prepares slurry, is made with spray dryer
After grain, drying, the powder is burnt into 2 hours with 800 DEG C of nitrogen streams, with the sieve of #100, yttrium fluoride (average grain diameter is made
37 μm) powder, obtain spraying plating powder.The spraying plating is L with powder*a*b*L in chrominance representation*: 58.46, a*: 3.63, b*: 2.85
Grey, the concentration of carbon in powder are 1.34%.In addition, oxygen concentration is 2.0%.The X-ray diffraction of powder, result viewing are carried out
To YF3And Y5O4F7Peak.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 37.78, a*: -0.06, b*: 5.76,
Concentration of carbon is 0.098%.In addition, oxygen concentration is 3.26%.The X-ray diffraction of envelope, result viewing to YF are carried out3With
Y5O4F7Peak.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[embodiment 5]
In white aluminium oxide (3 μm of average grain diameter) powder 100g and yttrium fluoride (3 μm of average grain diameter) powder 900g
4 liters of 3% aqueous solution of acrylic binder is added and mixes, prepares slurry, after being granulated with spray dryer, being dry, uses #
Yttrium fluoride (30 μm of average grain diameter) powder is made in 100 sieve, has obtained the spraying plating powder that oxygen concentration is 4.7%.The spray
Plating is L with powder*a*b*L in chrominance representation*: 90.24, a*: 4.60, b*: -5.55 white, the concentration of carbon in powder are 1.46%.
In addition, having carried out the X-ray diffraction of powder, result viewing to YF3And Al2O3Peak.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 27.75, a*: 2.96, b*: 0.64,
Concentration of carbon is 0.13 mass %, oxygen concentration 4.9%.In addition, having carried out the X-ray diffraction of envelope, result viewing to Y6O5F8With
Y3Al5O12(YAG) peak.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[embodiment 6]
In white yttrium oxide (0.2 μm of average grain diameter) powder 50g, white aluminium oxide (3 μm of average grain diameter) powder
4 liters of 0.2% aqueous solution of CMC binder is added in last 50g and yttrium fluoride (3 μm of average grain diameter) powder 900g and mixes, preparation slurry
The powder after being granulated with spray dryer, being dry, is burnt into 2 hours, with the sieve mistake of #100 by material with 1000 DEG C of nitrogen streams
Sieve, is made yttrium fluoride (30 μm of average grain diameter) powder, has obtained the spraying plating powder that oxygen concentration is 3.4%.The spraying plating is L with powder*a*
b*L in chrominance representation*: 89.52, a*: -0.07, b*: 1.92 white, the concentration of carbon in powder are 0.004%.Powder is carried out
X-ray diffraction, result viewing to Y7O6F9+Y3Al5O12(YAG) peak.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, result L*: 89.75, a*: -0.23, b*: 0.73,
Concentration of carbon is 0.009 mass %, oxygen concentration 3.8%.In addition, having carried out the X-ray diffraction of envelope, result viewing to Y6O5F8
And Y3Al5O12(YAG) peak.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[comparative example 3]
Using yttrium fluoride (30 μm of average grain diameter) powder of the oxygen containing 3%, sprayed using argon gas, hydrogen by plasma
Plating makes film be attached to aluminium alloy element to become the envelope of about 200 μ m-thicks.Determine the sprayed L*a*b*Coloration, as a result
For L*: 87.83, a*: -0.07, b*: 1.92, concentration of carbon is 0.003% or less.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test similarly to Example 3.Taking-up it is sprayed in see
Having arrived partly discoloration is dark brown and black part.
[embodiment 7]
1.5 liters of polyvinyl alcohol (PVA) 3% aqueous solution, chlorination are added in the yttrium fluoride powder 1kg that oxygen concentration is 12.8%
Titanium (TiCl3) 1.5g, it mixes, slurry is made, be granulated using spray dryer, be dry, having obtained pelletizing.While flowing argon gas
While the pelletizing is burnt into 1 hour at 1000 DEG C.By the sieve of obtained spraying plating powder #200, spraying plating use is made
Powder.Determine the L of the spraying plating powder*a*b*Coloration, result L*: 38.21, a*: 0.12, b*: 0.23 black powder, in powder
Titanium concentration is 680ppm.In addition, oxygen concentration is 13.1%.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the L of the envelope*a*b*Coloration, result L*: 41.02, a*: -0.56, b*: 4.31.Again
Have, the titanium concentration of envelope is 670ppm, oxygen concentration 13.5%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[embodiment 8]
1.5 liters of polyvinyl alcohol (PVA) 2% aqueous solution, molybdenum chloride are added in the yttrium fluoride powder 1kg that oxygen concentration is 2%
(MoCl5) 2.0g, it mixes, slurry is made, be granulated using spray dryer, be dry, having obtained pelletizing.When flowing argon gas
The pelletizing is burnt into 1 hour at 1000 DEG C.By the sieve of obtained spraying plating powder #200, spraying plating powder is made.
Determine the L of the spraying plating powder*a*b*Coloration, result L*: 45.23, a*: -0.08, b*: -0.21 black powder, in powder
Molybdenum concentration is 920ppm.In addition, oxygen concentration is 1.8%.
Using the spraying plating powder, using argon gas, hydrogen by plasma spraying make film be attached to aluminium alloy element at
It is the envelope of about 200 μ m-thicks.Determine the L of the envelope*a*b*Coloration, result L*: 63.82, a*: -0.47, b*: 0.75.Again
Have, the molybdenum concentration of envelope is 890ppm, oxygen concentration 2.5%.
The spraying plating component is set to reactive ion plasma experimental rig together with the silicon wafer for being coated with resist,
Using frequency 13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas
The condition of pressure 50mtorr has carried out plasma exposure test.The sprayed color taken out does not change.
[embodiment 9,10, comparative example 4,5]
The lanthanum fluoride that the gadolinium fluoride for the use of oxygen concentration being 0.48% (27.8 μm of average grain diameter) and oxygen concentration are 0.148%
(30.9 μm of average grain diameter), prepares pelletizing shown in table 1, is burnt into 2 hours, is obtained using firing condition shown in table 1
Spraying plating powder with carbon content shown in table 1, oxygen content and coloration.Next, using obtained spraying plating powder, with reality
It applies example 1 and is similarly formed on aluminium alloy element surface sprayed, obtain with carbon content shown in table 1, oxygen content and color
That spends is sprayed, carries out plasma exposure test similarly to Example 1, determines the coloration of envelope.It shows the result in
In table 1.
[table 1]
As was the case with table 1, implement firing (embodiment 9,10) in inert atmosphere, thus inhibit the reduction of carbon amounts, it can
Remain to 0.01% or more.On the other hand, if being burnt into (comparative example 4,5) in an atmosphere, carbon is reduced due to oxidation
To less than 0.01%, through spraying plating, the color of envelope becomes white.
[experimental example]
Use white yttrium oxide (0.2 μm of average grain diameter) powder 100g and yttrium fluoride (3 μm of average grain diameter) powder
900g and CMC as carbon source, has obtained 7 kinds of different spraying plating powder of concentration of carbon shown in table 2.In this case, sample
The spraying plating of product 6 is not to be burnt into powder using prepared by the method according to embodiment 3 with powder, the spraying platings of other samples with powder be using by
According to the firing powder of the method preparation of above-described embodiment 4.Next, being formd in table 2 with powder in aluminium alloy element using each spraying plating
Shown in about 200 μ m-thicks envelope.Each sprayed surface hardness (HV) and section measured using following methods is hard
It spends (HV), has studied carbon content and the relationship by film hardness.It shows the result in the coordinate diagram of table 2 and Fig. 2.
(measuring method of hardness)
For obtained each component, the test piece of 10mm square is made by cutting off processing.Mirror surface essence is carried out to surface, section
It processes (Ra=0.1 μm), implements the Determination of Hardness of envelope surface and section using Vickers.Use Vickers
(Akashi AVK-C1) carries out Determination of Hardness when load load 300gf, duration of load application 10 seconds, 3 points of surface hardness of measurement and
3 points of section hardness, its average value is evaluated.
[table 2]
As shown in table 2 and Fig. 2, if carbon content is more than 0.15 mass %, the hardness of envelope is reduced, if carbon
Content is 0.15 mass % or less, particularly 0.1 mass % hereinafter, confirmation obtains being more than the good by film hardness of 300HV.Cause
This, need height by film hardness in the case where, preferably make carbon content become 0.15 mass % or less, particularly 0.1 mass % with
Under.
[embodiment 11~14]
Using each powder of fluorination ytterbium, yttrium fluoride, gadolinium fluoride shown in table 3, similarly to Example 1 to aluminium alloy structure
Part carries out plasma spraying, forms sprayed shown in table 3.It is sprayed for what is obtained, using frequency
13.56MHz, plasma output power 1000W, gas kind CF4+O2(20 volume %), flow 50sccm, gas pressure
The condition of 50mtorr implements plasma exposure processing, has obtained with the sprayed of coloration shown in table 3.
[table 3]
As shown in table 3, by utilizing plasma light and etching gas to common white rare earth fluoride spraying plating
Envelope carries out plasma exposure processing, so as to obtain in the sprayed of uniform black.Moreover, this will be formd
In the case that the sprayed component of black is used as the anti-plasma member in halogen gas, the variation of the color of part
It is few, it also need not partly implement the cleaning for being difficult to carry out again when taking out cleaning, can certainly realize the long-life of script.
It is sprayed for black obtained in embodiment 12, the grinding of component surface ball is carried out, forms 1650 μm of diameter
Round pool, the measurement of the calculating formula according to shown in Fig. 1, the thickness for calculating black layer, result is 2 μm hereinafter, presumption is about
1000nm。
Claims (22)
1. sprayed, which is characterized in that be include following (1) and/or (2) or following (1) and/or (2) with selected from following
(3) one kind or two or more mixture in~(5) it is sprayed,
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
Carbon containing 0.004~2 mass % or titanium or molybdenum containing 1~1000ppm, and
In the case where the oxygen fluoride without (2), L is used*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+
5.0、b*Grey or even black for -6.0~+8.0,
Comprising the oxygen fluoride of (2), L is used*a*b*Chrominance representation is in L*It is 25 or more and less than 91, a*For-
3.0~+5.0, b*For -6.0~+8.0 white or grey or even black.
2. according to claim 1 sprayed, wherein rare earth element is selected from one or more of Y, Gd, Yb, La.
3. according to claim 1 or 2 sprayed, wherein oxygen content is 0.01~13.5 mass %.
4. described in any one of claim 1 to 3 sprayed, wherein carbon content is 0.004~0.15 mass %.
5. spraying plating powder, which is characterized in that be include following (1) and/or (2) or following (1) and/or (2) with selected from following
(3) the spraying plating powder of the one kind or two or more mixture in~(6),
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In
Carbon containing 0.004~2 mass % or titanium or molybdenum containing 1~1000ppm, and use L*a*b*Chrominance representation is in L*
It is 25 or more and less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even black.
6. spraying plating powder according to claim 5, wherein rare earth element is selected from one or more of Y, Gd, Yb, La.
7. spraying plating powder according to claim 5 or 6, wherein oxygen content is 0.01~13.5 mass %.
8. the spraying plating powder according to any one of claim 5~7, is the spraying plating powder through being burnt into, carbon content is
0.004~0.15 mass %.
9. the spraying plating powder according to any one of claim 5~7, for the spraying plating powder not being burnt into, carbon content is
0.004~1.5 mass %.
10. the manufacturing method of spraying plating powder is the method for manufacturing the spraying plating powder according to any one of claim 5~8,
It is characterized in that, will include following (1) and/or (2) or following (1) and/or (2) and a kind in following (3)~(6)
Or the white powder of mixture of more than two kinds is used in such a way that the concentration of carbon of spraying plating powder becomes 0.004~2 mass %
Carbon source slurry is dry, roasting, firing, obtain using L*a*b*Chrominance representation is in L*It is 25 or more and less than 91, a*For -3.0~+
5.0、b*For -6.0~+8.0 white or grey or even the spraying plating powder of black,
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In.
11. the manufacturing method of spraying plating powder according to claim 10, wherein carried out at 500~800 DEG C in nitrogen
After roasting, the powder being fired is burnt at 800~1000 DEG C in vacuum or non-active gas atmosphere.
12. the manufacturing method of spraying plating powder described in 0 or 11 according to claim 1, wherein including (1) and/or (2) or
(1) and/or (2) described in person and the oxygen of the white powder of the one kind or two or more mixture in (3)~(6) contain
Amount is 0.01~13.5 mass %.
13. the manufacturing method of spraying plating powder described in any one of 0~12 according to claim 1, wherein with the carbon of spraying plating powder
Concentration uses carbon source as the mode of 0.004~0.15 mass %.
14. the manufacturing method of spraying plating powder is the method for manufacturing the spraying plating powder according to any one of claim 5~8,
It is characterized in that, will include following (1) and/or (2) or following (1) and/or (2) and a kind in following (3)~(6)
Or the white powder of mixture of more than two kinds, polyvinyl alcohol, 1~1000ppm become with the concentration of the titanium of spraying plating powder or molybdenum
The slurry granulating and drying of the water soluble salt of titanium or molybdenum that uses of mode, firing, obtain using L*a*b*Chrominance representation is in L*For 25 with
Above and less than 91, a*For -3.0~+5.0, b*For -6.0~+8.0 white or grey or even the spraying plating powder of black,
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In.
15. the manufacturing method of spraying plating powder according to claim 14, wherein in vacuum or non-active gas atmosphere
The powder through granulating and drying is burnt at 800~1000 DEG C.
16. the manufacturing method of spraying plating powder according to claim 14 or 15, wherein including (1) and/or (2) or
(1) and/or (2) described in person and the one kind or two or more mixture in (3)~(6) include mixture in white
The oxygen content of the powder of color is 0.01~13.5 mass %.
17. sprayed, which is characterized in that be to include following (1) and/or (2) or following (1) and/or (2) and be selected from down
The sprayed of the one kind or two or more mixture in (3)~(5) is stated, has on surface and uses L*a*b*Chrominance representation is in L*For
25~64, a*For -3.0~+5.0, b*For -6.0~+8.0 grey or even the grey of black or even black layer,
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In.
18. according to claim 17 sprayed, wherein grey or even the depth of black layer are 2 μ away from envelope surface
Within m.
19. sprayed described in 7 or 18 according to claim 1, wherein oxygen content is 0.01~13.5 mass %.
20. sprayed manufacturing method is manufacturer sprayed described in any one of 7~19 according to claim 1
Method, which is characterized in that will be including following (1) and/or (2) or following (1) and/or (2) and in following (3)~(6)
The white powder of one kind or two or more mixture obtains using L to substrate surface spraying plating*a*b*Chrominance representation is in L*For 81 with
Upper, a*For -3.0~+3.0, b*For -3.0~+3.0 white it is sprayed, to the sprayed implementation plasma exposure
Processing forms on the sprayed surface and uses L*a*b*Chrominance representation is in L*For 25~64, a*For -3.0~+5.0, b*For -6.0~
+ 8.0 grey or even the grey of black or even black layer,
(1) fluoride of the rare earth element selected from one or more of the rare earth element of 3A race comprising yttrium
(2) oxygen fluoride of the rare earth element
(3) oxide of the rare earth element
(4) composite oxides of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(5) composite fluoride of the rare earth element and the one kind or two or more metal in Al, Si, Zr, In
(6) oxide of the one kind or two or more metal in Al, Si, Zr, In.
21. sprayed manufacturing method according to claim 20, wherein making the depth of grey or even black layer becomes
Within 2 μm away from envelope surface.
22. the manufacturing method of spraying plating powder according to claim 20 or 21, wherein including (1) and/or (2) or
(1) and/or (2) described in person and the oxygen of the white powder of the one kind or two or more mixture in (3)~(6) contain
Amount is 0.01~13.5 mass %.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211112737.3A CN115354269A (en) | 2017-03-01 | 2018-02-28 | Thermal spray coating, thermal spray powder, method for producing thermal spray powder, and method for producing thermal spray coating |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017038174 | 2017-03-01 | ||
| JP2017-038174 | 2017-03-01 | ||
| PCT/JP2018/007624 WO2018159713A1 (en) | 2017-03-01 | 2018-02-28 | Spray coating, spraying powder, spraying powder manufacturing method and spray coating manufacturing method |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211112737.3A Division CN115354269A (en) | 2017-03-01 | 2018-02-28 | Thermal spray coating, thermal spray powder, method for producing thermal spray powder, and method for producing thermal spray coating |
Publications (2)
| Publication Number | Publication Date |
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| CN110382730A true CN110382730A (en) | 2019-10-25 |
| CN110382730B CN110382730B (en) | 2022-09-23 |
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| CN202211112737.3A Pending CN115354269A (en) | 2017-03-01 | 2018-02-28 | Thermal spray coating, thermal spray powder, method for producing thermal spray powder, and method for producing thermal spray coating |
| CN201880014710.6A Active CN110382730B (en) | 2017-03-01 | 2018-02-28 | Thermal spray coating, thermal spray powder, method for producing thermal spray powder, and method for producing thermal spray coating |
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Country Status (6)
| Country | Link |
|---|---|
| US (2) | US20200002799A1 (en) |
| JP (1) | JP6436270B1 (en) |
| KR (3) | KR102536087B1 (en) |
| CN (2) | CN115354269A (en) |
| TW (2) | TWI807631B (en) |
| WO (1) | WO2018159713A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115926496A (en) * | 2022-11-09 | 2023-04-07 | 三明宝氟新材料科技有限公司 | Yttrium fluoride spraying material |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7124798B2 (en) * | 2018-07-17 | 2022-08-24 | 信越化学工業株式会社 | Membrane-forming powder, method for forming coating, and method for producing membrane-forming powder |
| JP2021155784A (en) * | 2020-03-26 | 2021-10-07 | トヨタ紡織株式会社 | Method for producing metal nanoparticles, method for producing membrane electrode assembly, and method for producing solid polymer electrolyte fuel cell |
| JP2022083511A (en) | 2020-11-25 | 2022-06-06 | 三星電子株式会社 | Sintered body, method of producing sintered body, semiconductor production device, and method of producing semiconductor production device |
| KR20240030718A (en) | 2022-08-31 | 2024-03-07 | (주)코미코 | Yttrium-based powder for thermal spraying and yttrium-based thermal spray coating using the same |
| CN115861721B (en) * | 2023-02-28 | 2023-05-05 | 山东大佳机械有限公司 | Livestock and poultry breeding spraying equipment state identification method based on image data |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN115354269A (en) | 2022-11-18 |
| TWI807631B (en) | 2023-07-01 |
| JP6436270B1 (en) | 2018-12-12 |
| US20240102142A1 (en) | 2024-03-28 |
| KR102664599B1 (en) | 2024-05-14 |
| CN110382730B (en) | 2022-09-23 |
| JPWO2018159713A1 (en) | 2019-03-07 |
| WO2018159713A1 (en) | 2018-09-07 |
| KR102536087B1 (en) | 2023-05-24 |
| US20200002799A1 (en) | 2020-01-02 |
| KR20230076868A (en) | 2023-05-31 |
| TWI756374B (en) | 2022-03-01 |
| KR20240067976A (en) | 2024-05-17 |
| TW201842210A (en) | 2018-12-01 |
| TW202218872A (en) | 2022-05-16 |
| KR20190122753A (en) | 2019-10-30 |
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